反应 #76331

反应方程式

3-bromo-4-fluorobenzaldehyde

morpholine

K2CO3

→

3-bromo-4-(4-morpholinyl)benzaldehyde

收率 58.2%

溶剂

pyridine

反应条件

后处理

1. 1
   温度the slurry was refluxed for 18 h
2. 2
   其他The solvent was removed
3. 3
   其他the residue was partitioned between ethyl acetate and water
4. 4
   其他The organic layer was separated
5. 5
   干燥dried (MgSO4)
6. 6
   其他evaporated to a yellow oil
7. 7
   其他Purification by flash chromatography on silica gel eluting with 15% ethyl acetate in hexane

实验过程

Ex-604A) To a pyridine (15 mL) solution of 3-bromo-4-fluorobenzaldehyde (1.0 g, 4.9 mmol) was added morpholine (0.5 mL, 5.7 mmol) and K2CO3 (0.69 g, 5.0 mmol), and the slurry was refluxed for 18 h. The solvent was removed, and the residue was partitioned between ethyl acetate and water. The organic layer was separated, dried (MgSO4) and evaporated to a yellow oil. Purification by flash chromatography on silica gel eluting with 15% ethyl acetate in hexane gave 0.77 g (58%) of the desired 3-bromo-4-(4-morpholinyl)benzaldehyde product as an white solid. 1H NMR (CDCl3) δ3.18 (m, 4H), 3.90 (m, 4H), 7.10 (d, 1H), 7.78 (d, 1H), 8.07 (s, 1H), 9.83 (s, 1H).

来源